Abstract: The Weinreb amides 2a, b were prepared from the α, α-dimethoxyacetic acids 1c, d. A number of representative nucleophilic additions (RMgX and RLi) on 2 afforded α- ketoacetals 3a–j in 70–99% yield. These compounds represent a versatile arrangement of functional groups of significant synthetic value, as demonstrated in the synthesis of (±)- salbutamol.